B200-17 Sodium Chloride.pdf

AWWA Standard

SM

Sodium Chloride

Effective date May 1, 2017.

First edition approved by AWWA Board of Directors July 6, 1949.

This edition approved Jan. 14, 2017.

Approved by American National Standards Institute Jan. 24, 2017.

ANSI/AWWA B200-17

(Revision of ANSI/AWWA B200-12)

Copyright © 2017 American Water Works Association. All Rights Reserved.

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AWWA Standard This document is an American Water Works Association (AWWA) standard. It is not a specification. AWWA standards describe minimum requirements and do not contain all of the engineering and administrative information normally contained in specifications. The AWWA standards usually contain options that must be evaluated by the user of the standard. Until each optional feature is specified by the user, the product or service is not fully defined. AWWA pub-lication of a standard does not constitute endorsement of any product or product type, nor does AWWA test, certify, or approve any product. The use of AWWA standards is entirely voluntary. This standard does not supersede or take precedence over or displace any applicable law, regulation, or code of any governmental authority. AWWA standards are intended to represent a consensus of the water industry that the product described will provide satisfactory ser-vice. When AWWA revises or withdraws this standard, an official notice of action will be placed on the first page of the Official Notice section of Journal – American Water Works Association. The action becomes effective on the first day of the month following the month of Journal – American Water Works Association publication of the official notice.

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An American National Standard is intended as a guide to aid the manufacturer, the consumer, and the general public.

The existence of an American National Standard does not in any respect preclude anyone, whether that person has approved the standard or not, from manufacturing, marketing, purchasing, or using products, processes, or proce-dures not conforming to the standard. American National Standards are subject to periodic review, and users are cau-tioned to obtain the latest editions. Producers of goods made in conformity with an American National Standard are encouraged to state on their own responsibility in advertising and promotional materials or on tags or labels that the goods are produced in conformity with particular American National Standards.

Caution Notice: The American National Standards Institute (ANSI) approval date on the front cover of this standard indicates completion of the ANSI approval process. This American National Standard may be revised or withdrawn at any time. ANSI procedures require that action be taken to reaffirm, revise, or withdraw this standard no later than five years from the date of publication. Purchasers of American National Standards may receive current information on all standards by calling or writing the American National Standards Institute, 25 West 43rd Street, Fourth Floor, New York, NY 10036; 212.642.4900; or emailing info@ansi.org.

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ISBN-13, print: 978-1-58321-214-6 eISBN-13, electronic: 978-1-61300-414-2

DOI: http://dx.doi.org/10.12999/AWWA.B200.17

All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopy, recording, or any information or retrieval system, except in the form of brief excerpts or quotations for review purposes, without the written permission of the publisher.

Copyright © 2017 by American Water Works Association Printed in USA iii

Committee Personnel

The AWWA Standards Committee on Ion Exchange, which reviewed and approved this standard, had the following personnel at the time of approval:

Todd M. Minten, Chair

General Interest Members

Producer Members

User Members

* Liaison, nonvoting

This page intentionally blank.

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Contents All AWWA standards follow the general format indicated subsequently. Some variations from this format may be found in a particular standard.

SEC. PAGE SEC. PAGE

Foreword I Introduction..................................... vii

I.A Background...................................... vii

I.B History............................................ viii

I.C Acceptance........................................ ix

II Special Issues...................................... x

III Use of This Standard.......................... x

III.A Purchaser Options and Alternatives.................................. x

III.B Modification to Standard.................. xi

IV Major Revisions................................. xi

V Comments........................................ xi

Standard

1 General

1.1 Scope

1.2 Purpose

1.3 Application

2 References

3 Definitions

4 Requirements

4.1 Physical Requirements

4.2 Chemical Requirements

4.3 Impurities

5 Verification

5.1 Inspection

5.2 Sampling

5.3 Test Procedures—General

5.4 Moisture

5.5 Insoluble Matter

5.6 Calcium

5.7 Magnesium

5.8 Sulfate

5.9 Grease, Fat, and Oil

5.10 pH Value

5.11 Total Impurities

5.12 Sodium Chloride Assay

5.13 Notice of Nonconformance

6 Delivery

6.1 Marking

6.2 Packaging and Shipping

6.3 Affidavit of Compliance

Table 1 Maximum Impurity Limits vii

Foreword This foreword is for information only and is not a part of ANSI*/AWWA B200.

have evaporated. Bedded deposits occur in horizontal layers of the mineral halite. These layers range from several feet to hundreds of feet (meters) in thickness and are between several feet and several thousand feet (meters) below the surface of the earth. Some bedded deposits between 25,000 ft and 50,000 ft (7,600 m and 15,200 m) below the surface of the earth have been subjected to pressures that have caused the salt to move upward through overlying sedimentary layers toward the Earth’s surface. Presently, these deposits exist as domes of nearly pure salt that may be as large as 2 mi (3.2 km) in diameter and are sometimes found within a few feet of the Earth’s surface.

Concentrated brine† is found in surface lakes or underground pools. Along sea-coasts, the oceans provide a virtually unlimited source of salt.

Rock salt is produced by the conventional room-and-pillar mining method. After sinking a shaft to the salt level, the face, or vertical area, is drilled and may be under-cut. The drill holes are loaded with explosives, and the explosives are detonated. The fragmented salt that results is crushed, screened, transported to the shaft, and hoisted to the surface.

Solar salt is produced by the natural evaporation of seawater or more concentrated brine from surface lakes or underground formations in shallow ponds.

Solution-mined brine, from which evaporated salt is produced, is obtained by drill-ing wells into bedded or domal rock-salt deposits and injecting water into the deposit.

The water dissolves the rock salt to produce a saturated brine. Salt deposits can be solution-mined through a single set of concentric pipes or through two or more sepa-rate pipes within the same deposit. The brine can then be evaporated to produce dry salt by vacuum-pan evaporation or modifications of vacuum-pan evaporation, grainer evaporation, or the Alberger process.

In vacuum-pan evaporation, cubic “vacuum-granulated” salt crystals form in the brine during evaporation and are removed as a slurry, which is then dewatered and dried.

viii

In the grainer process, small hoppers of salt form on the surface of a concentrated brine solution. These drop to the bottom of the grainer pan once they become large enough to overcome forces that hold them to the surface. The resultant flake salt is removed from the grainer by rakes and dried in a rotary dryer.

The Alberger process is a part vacuum-pan, part grainer operation in which cubic crystals are formed in a flash chamber and fed to the grainer pans. The seed crystals in the grainer pan produce a product that is a mixture of grainer-type flakes and flakes grown on seed crystals. The salt is centrifuged from the brine and dried as in the grainer process. Screens are used to separate the salt into specific grades.

Any of the three salt types (rock, solar, or vacuum-granulated and their compressed forms) can be used for regeneration of ion-exchange resins. The greater quantity of insoluble matter in some rock salt may require clarification of the brine. The accumula-tion of insolubles in the brine tank is a disadvantage because periodic removal is neces-sary. Vacuum-granulated salt has the highest purity and leaves no insoluble residue.

Salt for regeneration of ion-exchange units should be selected on the basis of the brine purity required. Cation-exchange processes usually require that the saturated brine contain less than 2,000 mg/L of calcium sulfate (CaSO4). Anion-exchange pro-cesses require brine with low calcium and magnesium (Mg) content to produce a con-sistent quality of effluent water. When caustic soda or soda ash is added to the brine makeup, saturated brine with a calcium level of 0 to 10 mg/L (as Ca) should be used.

The magnesium level should be 0 to 2 mg/L (as Mg).

I.B. History. The first edition of the AWWA standard for sodium chloride was approved as tentative by the AWWA Board of Directors on July 6, 1949. ANSI/ AWWA B200 was made a standard on May 15, 1953. Revisions approved on June 5, 1964, provided new sections on information to be supplied by the purchaser and on an affidavit of compliance. The revisions also provided for the use of the ethylenediaminetetraacetic acid (EDTA) titrimetric method for determining calcium and magnesium, the permanganate titrimetric method for calcium, and the gravimetric method for magnesium.

The 1969 revisions of the standard provided for two types of salt that were not included in earlier standards: evaporated and compressed evaporated salt. At that time, the impurity limits for certain constituents were revised, the definitions section was revised and enlarged, the physical characteristics were modified regarding fineness requirements, and minor changes were made in the test methods. The 1978 edition combined evaporated salt and compressed evaporated salt and added a specification for compressed solar salt. The 1988 edition included an acceptance clause in the fore-ix word and revised definitions, limits, and test procedures. The 1993 edition included a revised acceptance statement and definitions. The 1998 edition of ANSI/AWWA B200 was revised to conform to AWWA standard style. The ninth edition of ANSI/AWWA B200 was approved by the AWWA Board of Directors on June 11, 2006. The last revi-sion was approved on Jan. 22, 2012. This edition was approved on Jan. 14, 2017.

I.C. Acceptance. In May 1985, the US Environmental Protection Agency (USEPA) entered into a cooperative agreement with a consortium led by NSF International (NSF) to develop voluntary third-party consensus standards and a certification program for direct and indirect drinking water additives. Other members of the original consortium included the Water Research Foundation (formerly AwwaRF), and the Conference of State Health and Environmental Managers (COSHEM). The American Water Works Association (AWWA) and the Association of State Drinking Water Administrators (ASDWA) joined later.

In the United States, authority to regulate products for use in, or in contact with, drinking water rests with individual states.* Local agencies may choose to impose requirements more stringent than those required by the state. To evaluate the health effects of products and drinking water additives from such products, state and local agencies may use various references, including two standards developed under the direction of NSF:† NSF/ANSI 60, Drinking Water Treatment Chemicals—Health Effects, and NSF/ANSI 61, Drinking Water System Components—Health Effects.

Various certification organizations may be involved in certifying products in accor-dance with NSF/ANSI 60. Individual states or local agencies have authority to accept or accredit certification organizations within their jurisdictions. Accreditation of certi-fication organizations may vary from jurisdiction to jurisdiction.

Annex A, “Toxicology Review and Evaluation Procedures,” to NSF/ANSI 60 does not stipulate a maximum allowable level (MAL) of a contaminant for substances not regulated by a USEPA final maximum contaminant level (MCL). The MALs of an unspecified list of “unregulated contaminants” are based on toxicity testing guidelines (noncarcinogens) and risk characterization methodology (carcinogens). Use of Annex A procedures may not always be identical, depending on the certifier.

ANSI/AWWA B200 addresses additives requirements in Sec. 4.3 of the standard.

The transfer of contaminants from chemicals to processed water or to residual solids is becoming a problem of great concern. The language in Sec. 4.3.4 is a recommenda-

x tion only for direct additives used in the treatment of potable water to be certified by an accredited certification organization in accordance with NSF/ANSI 60, Drinking Water Treatment Chemicals—Health Effects. However, users of the standard may opt to make this certification a requirement for the product. Users of this standard should consult the appropriate state or local agency having jurisdiction in order to

ucts for contact with, or treatment of, drinking water.

3. Determine current information on product certification.

II. Special Issues. Currently, there are no special issues related to this standard.

III. Use of This Standard. It is the responsibility of the user of an AWWA standard to determine that the products described in that standard are suitable for use in the particular application being considered.

III.A. Purchaser Options and Alternatives. The following information should be provided by the purchaser:

1. Standard used—that is, ANSI/AWWA B200, Sodium Chloride, of latest revision.

2. Whether compliance with NSF/ANSI 60, Drinking Water Treatment Chemicals—Health Effects, is required.

3. When rock salt is readily available with values for moisture, calcium, mag-nesium, sulfates, or water-insoluble impurities lower than those shown in Table 1 of the standard, purchasers may prefer to modify the limits set in the table for these sub-stances (Sec. 4.3.2).

4. Details of other federal, state or provincial, and local requirements (Sec. 4.3.3 and Sec. 6.2).

5. Whether the purchaser will reject product from containers or packaging with missing or damaged seals. The purchaser may reject product from bulk containers or packages with missing or damaged seals unless the purchaser’s tests of representative samples, conducted in accordance with Sec. 5.3, demonstrate that the product meets the standard. Failure to meet the standard or the absence of, or irregularities in, seals may be sufficient cause to reject a shipment.

6. Quantity of sodium chloride required and method of packaging and ship-ping (Sec. 6.2).

7. Whether bulk shipments of sodium chloride are accompanied by weight certificates of certified weighers (Sec. 6.2.4).

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8. Whether alternative security measures have been adopted to replace or aug-ment the security measures set out in Sec. 6.2.5 and 6.2.6.

or terminology in this standard must be provided by the purchaser.

IV. Major Revisions. Major changes made to the standard in this revision include the following:

provided by the manufacturer of the product and not the supplier.

V. Comments. If you have any comments or questions about this standard, please call AWWA Engineering and Technical Services at 303.794.7711, FAX at 303.795.7603; write to the department at 6666 West Quincy Avenue, Denver, CO 80235-3098; or email at standards@awwa.org.

AWWA Standard®

ANSI/AWWA B200-17

(Revision of ANSI/AWWA B200-12)

Sodium Chloride

SECTION 1: GENERAL

Sec. 1.1 Scope This standard describes sodium chloride in the forms of rock, vacuum-gran-ulated, compressed vacuum-granulated, solar, and compressed solar salt for use in the recharging of cation-exchange materials in water supply service for softening municipal and industrial potable water, wastewater, and reclaimed water supplies.

Additionally, sodium chloride is used in the recharging of anion-exchange materi-als for nitrate removal or dealkalization of municipal and industrial supplies.

Sec. 1.2 Purpose The purpose of this standard is to provide the minimum requirements for sodium chloride, including physical, chemical, sampling, packaging, shipping, and testing requirements.

Sec. 1.3 Application This standard can be referenced in the purchaser’s documents for purchasing and receiving sodium chloride and can be used as a guide for testing the physi-cal and chemical properties of sodium chloride samples. The stipulations of this standard apply when this document has been referenced and then only to sodium chloride used in the treatment of potable water, wastewater, or reclaimed water.

2 AWWA B200-17

SECTION 2: REFERENCES

This standard references the following documents. In their latest editions, they form a part of this standard to the extent specified within the standard. In any case of conflict, the requirements of this standard shall prevail.

APHA,* AWWA, and WEF.† Standard Methods for the Examination of Water and Wastewater. Washington, D.C.: APHA, AWWA, and WEF.

ASTM‡ E11—Standard Specification for Woven Wire Test Sieve Cloth and Test Sieves.

NSF§/ANSI¶ 60—Drinking Water Treatment Chemicals—Health Effects.

USDHHS-NIOSH** Publication No. 81-123—Occupational Health Guide-lines for Chemical Hazards, Section on 1,1,2-Trichloro-1,2,2-Trifluoroethane.

SECTION 3: DEFINITIONS

The following definitions shall apply in this standard:

1. Compressed salt: A product made into various sizes and shapes by mechanically compressing vacuum-granulated or solar salt.

2. Day: A day is defined as a 24-hour period.

3. Manufacturer: The party that manufactures, fabricates, or produces materials or products.

4. Potable water: Water that is safe and satisfactory for drinking and cooking.

5. Purchaser: The person, company, or organization that purchases any materials or work to be performed.

6. Reclaimed water: Wastewater that becomes suitable for beneficial use as a result of treatment.

7. Rock salt: A mined salt that is crushed and screened.

8. Salt: A stable compound with the chemical formula NaCl.

Columbia Parkway Cincinnati, OH 45226.

Sodium Chloride 3

9. Solar salt: Salt produced by evaporating, via the action of sun and wind, seawater, lake brine, or saline groundwater in shallow ponds.

10. Supplier: The party that supplies materials or services. A supplier may or may not be the manufacturer.

11. Tamper-evident packaging: Packaging having one or more indicators or barriers to entry that if breached or missing, can reasonably be expected to provide visible evidence to the purchaser that tampering has occurred. The tamper-evident features of the packaging shall be designed to, and shall, remain intact when handled in a reasonable manner during manufacture, storage, shipment, and delivery to the purchaser. Properly constructed, labeled, closed, and sealed bags and trucks or trailers with locking devices constitute two effective forms of tamper-evident packaging.

12. Vacuum-granulated salt: Salt produced by evaporation of brine under special conditions designed to control crystal size and purity.

13. Wastewater: A combination of the liquid and water-carried waste from residences, commercial buildings, industrial plants, and institutions, together with any groundwater, surface water, and stormwater that may be present.

SECTION 4: REQUIREMENTS

Sec. 4.1 Physical Requirements

4.1.1 General. The material shall be homogenous and in a crystalline, granular, or compressed form.

4.1.2 Foreign matter. The material shall be free from dirt, fibers, lint, chips, trash, or other foreign matter.

4.1.3 Color. The material shall be white, grayish pink, brown, or brown-ish white, or of a distinguishing color added by the producer.

4.1.4 Fineness.*

4.1.4.1 Rock salt shall be of such fineness that 100 percent of it shall pass a ¾-in. (19-mm) sieve and not more than 5 percent of it shall pass a No. 60 (0.25-mm) sieve.

* Sieve numbers referred to in this standard are US Standard Sieve Series numbers, as specified in ASTM E11.

4 AWWA B200-17

4.1.4.2 Vacuum-granulated salt shall be of such fineness that 100 percent of it shall pass a No. 10 (2-mm) sieve and not more than 5 percent shall pass a No. 100 (0.15-mm) sieve.

4.1.4.3 Compressed vacuum-granulated and compressed solar salt shall be of such fineness that not more than 10 percent of it shall pass a No. 30 (0.59-mm) sieve.

4.1.4.4 Solar salt shall be of such fineness that 100 percent of it shall pass a 1¼-in. (31-mm) sieve and not more than 5 percent of it shall pass a No. 100 (0.15-mm) sieve.

Sec. 4.2 Chemical Requirements

4.2.1 NaCl content. The material shall have the following minimum NaCl content by weight (dry basis), as determined by the test methods given in Section 5:

rock salt, 96 percent; vacuum-granulated and compressed vacuum-granulated salt,

99.5 percent; and solar and compressed solar salt, 98 percent.

4.2.2 pH of solution. The solution formed by dissolving 10 g of the salt in 190 mL distilled water to make a 5 percent solution shall have a pH value greater than 5 and less than 9.5.

Sec. 4.3 Impurities*

4.3.1 General impurities. The sodium chloride supplied in accordance with this standard shall contain no soluble inorganic or organic substances in quantities capable of producing deleterious or injurious effects on the health of those consuming the water that has been properly treated by a material that has been properly regenerated with sodium chloride. The specified sodium chloride shall contain no contaminants that would cause treated water to fail to meet the requirements of US Environmental Protection Agency (USEPA) drinking water regulations. In addition, the sodium chloride shall contain no constituents that if released into treated water after regeneration and rinsing, will impair the useful-ness of the water for domestic consumption.

4.3.2 Specific impurity limits. The sodium chloride shall not exceed the maximum impurity limits listed in Table 1.

4.3.3 Regulatory requirements. Materials shall comply with the require-ments of the Safe Drinking Water Act and other federal regulations for potable water, wastewater, and reclaimed water systems, as applicable.

* See Sec. I.C of the foreword.

Sodium Chloride 5

4.3.4 Product certifications. Sodium chloride is a direct additive used in the treatment of potable water. This material should be certified as suitable for contact with, or treatment of, drinking water by an accredited certification organization in accordance with NSF/ANSI 60. Evaluation shall be accomplished in accordance with requirements that are no less restrictive than those listed in NSF/ANSI 60. Certification shall be accomplished by a certification organization accredited by the American National Standards Institute.

SECTION 5: VERIFICATION

Sec. 5.1 Inspection If desired by the purchaser, the shipment shall be inspected at the point of destination for evidence of foreign matter, such as dirt, fibers, lint, chips, or trash, that would be detrimental to the use of the salt.

Sec. 5.2 Sampling If an inspection is performed as specified in Sec. 5.1 and the shipment passes the inspection, sampling shall be as specified in this section.

5.2.1 Sampling. Samples shall be taken at the point of destination.

Table 1 Maximum impurity limits

Maximum Limit—Percent by Weight

Rock Salt

Vacuum- Granulated

Salt

Compressed Vacuum-

Granulated Salt Solar Salt

Compressed Solar Salt

Moisture 3.00 0.20 0.50 3.00 0.50

Dry Basis Water-soluble impurities Calcium and magnesium (Ca and Mg)

1.50 0.15 0.15 0.60 0.60

Sulfate (SO4) 3.00 0.35 0.35 1.40 1.40 Water-insoluble impurities 2.00 0.05 0.05 0.15 0.15 Total impurities (soluble + insoluble)

4.00 0.50 0.50 2.00 2.00

Grease, fat, or oil 0.01 0.01 0.01 0.01 0.01

6 AWWA B200-17

5.2.2 Number of packages. If the material is packaged, not less than 5 per-cent of the packages shall be sampled. No sample shall be taken from a broken package.

5.2.3 Bulk shipments. When delivered in bulk, the samples shall be repre-sentative of all parts of the bulk loads and shall not contain a disproportionate share of the top or bottom layers. Coarse material taken from bulk loads shall comprise at least 10 shovelfuls from different parts of the load, and the total material shall weigh not less than 100 lb (45 kg). The material shall be mixed and divided to make a sample of approximately 10 lb (4.5 kg) and handled as described in Sec. 5.2.5.

5.2.4 Device. Finely divided material, whether in bulk or packages, may be sampled using a sampling tube that is at least ¾ in. (19 mm) in diameter. Special precautions shall be used to avoid taking a disproportionate amount of the sample from the top or the bottom layers of the material. If the sodium chloride is handled by conveyor or elevator, a mechanical sampling arrangement may be used.

5.2.5 Handling. The gross sample, weighing at least 10 lb (4.5 kg), shall be thoroughly mixed and split to provide three 500-g material samples. Each mate-rial sample shall be sealed in an airtight, moisture-proof glass or plastic container.

Each sample container shall be labeled to identify it, and the label shall be signed by the sampler.

5.2.6 Test samples. One of the 500-g material samples (Sec. 5.2.5) shall be designated as the test sample for use by the purchaser. The two remaining mate-rial samples shall be retained for use according to Sec. 5.13, if necessary. Material samples shall be unsealed only when necessary to remove quantities of the material for testing.

Immediately before testing, the particles of the 500-g test sample may be reduced by mechanical grinding or by hand in a mortar to such size that all of it passes a No. 8 sieve. Samples selected for testing should be weighed rapidly to avoid changes in moisture content.

5.2.6.1 Rock, solar, and compressed solar salt.

50-g representative portion of solar or compressed solar salt.

3. Place 200 mL of distilled water in a two-speed blender and start at low speed.

4. Slowly add salt to blender and then blend for 5 minutes at high speed with cover in place.

Sodium Chloride 7

stock solution for subsequent analyses.

5.2.6.2 Vacuum-granulated and compressed vacuum-granulated salt.

insoluble calcium salts, particularly calcium carbonate (CaCO3).

5. Dilute to volume and mix to make stock solution for subsequent analyses.

Sec. 5.3 Test Procedures—General Sampling shall be conducted according to Sec. 5.2 of this standard. The pur-chaser shall complete the laboratory examination of the sample within five days after the shipment is received. Methods of testing sodium chloride shall conform to the procedures presented in the following sections. Alternative procedures shall only be used with the written approval of the purchaser. In any case of conflict, the methods of this standard shall prevail.

Sec. 5.4 Moisture

5.4.1 Procedure.

1. Weigh (to the nearest 0.01 g) 50 g of rock or solar salt or 100 g (to the nearest 0.01 g) of vacuum-granulated, compressed vacuum-granulated, or com-pressed solar salt, in an as-received condition, into a previously dried and tared moisture dish.

2. Place in an oven at 110°C. After 2 hours, remove to a desiccator; cool and weigh. Repeat until constant weight is obtained.

5.4.2 Calculation.

loss of weight × 100 = percent moisture (Eq 1) weight of sample

Sec. 5.5 Insoluble Matter

5.5.1 Procedure for rock, solar, and compressed solar salts.

1. Transfer a 200-mL prepared sample from Sec. 5.2.6.1(Item 6) to a 1-L

Erlenmeyer flask. Wash blender with 100 mL of distilled water. Add blender wash and 300 mL of distilled water to flask to obtain a total of 600 mL of water.

8 AWWA B200-17

2. Stir on a magnetic stirrer for 1 hour. Adjust the stirrer speed to give maxi-mum agitation without losing any sample as a result of splashing. Place beaker over the top of the flask while stirring.

3. Filter through a Gooch crucible and quantitatively recover insolubles on a previously dried (110°C for 1 hour) and weighed (analytical balance) glass-fiber filter paper or equivalent. Wash until free of chlorides as determined by testing small portions of filtrate with approximately N/10 silver nitrate (AgNO3). Filtrate tested should be disposed of separately, without combining with the total filtrate.

5.5.2 Procedure for vacuum-granulated and compressed vacuum-granulated salt.

through a Gooch crucible and quantitatively recover insolubles on a previously dried (110°C for 1 hour) and weighed (analytical balance) glass-fiber filter paper or equivalent. Wash until free of chlorides as determined by testing small portions of filtrate with approximately N/10 silver nitrate (AgNO3). The filtrate tested should be disposed of separately, without combining with the total filtrate.

procedures.

5.5.3 Calculation.

increase in weight of filter paper × 100 = percent of insoluble matter (dry basis) (Eq 2) grams per sample

Sec. 5.6 Calcium The test procedure for calcium uses the ethylenediaminetetraacetic acid

(EDTA) titrimetric method.

5.6.1 Reagents.

1. Sodium hydroxide solution, 1N. Dissolve 40 g NaOH (reagent grade) and dilute to 1 L with distilled water.

Sodium Chloride 9

2. Ammonium purpurate indicator. A ground mixture of the dry powder and sodium chloride provides a stable form of indicator. Mix 0.20 g ammonium purpurate (murexide) with 100 g of reagent-grade NaCl and grind the mixture to pass a No. 40 to No. 50 sieve.

3. EDTA titrant, 0.0100M. Dissolve 3.72 g of the reagent grade of the diso-dium salt of EDTA in 1,000 mL of distilled water. Standardize against standard calcium solution using the procedure described in Sec. 5.6.2. Standard EDTA titrant, exactly 0.0100M, is equivalent to 0.4008 mg Ca per 1.00 mL of titrant used. Titrant should be kept in heat-resistant glass or plastic bottles. Molarity M is used in the Sec. 5.6.3 calculation.

4. Standard calcium solution. Dry several grams of calcium carbonate pow-der (primary standard or special reagent low in heavy metals, alkalies, and mag-nesium) at 110°C overnight or longer. Weigh 1.000 g into a 500-mL Erlenmeyer flask. Slowly add 1:1 HCl until all the CaCO3 has dissolved. Add 200 mL of distilled water; boil to expel CO2. Cool, add a few drops of methyl red indicator, and adjust to the intermediate orange color by adding 3N NH4OH or 1:1 HCl, as required. Transfer quantitatively to a 1-L volumetric flask and fill to the mark with distilled water. This standard solution is equivalent to 0.4008 mg Ca per 1.00 mL.

Also, the standard solution is equivalent to 1.000 mg CaCO3 per 1.00 mL.

5.6.2 Procedure.

Note: Because the indicator is unstable at the high pH in this procedure, the titration should be performed immediately after adding indicator to the alkaline solution.

1. Pipette a 50- to 100-mL aliquot of stock into a separate 400-mL beaker for rock-salt analyses (depending on purity), 50 mL for vacuum-granulated and 100 mL for solar and compressed salt, so that the calcium content is 5 to 100 mg.

2. Dilute to 200 mL with water, if necessary. Add 2.0 mL 1N NaOH solu-tion or a volume sufficient to produce a pH of 12 to 13. Stir for a few minutes before titrating. The target pH for titration is 12.5, but this is measurable only with a “low-sodium error” glass electrode.

3. Add 0.1 to 0.2 g of the Sec. 5.6.1(Item 2) indicator mixture. Without delay, add EDTA titrant slowly and stir continuously until the color of the solu-tion changes from pink to purple at the end point. Record the milliliters of EDTA titrant and use for calculation (Sec. 5.6.3).

4. Check the end point by adding 1 or 2 drops of titrant in excess to make certain that no further color change takes place.

10 AWWA B200-17

5.6.3 Calculation.

M of EDTA × mL EDTA × 4.008 = percent calcium (Ca, dry basis) (Eq 3) grams of sample in aliquot

Sec. 5.7 Magnesium

5.7.1 Principle. Magnesium content can be determined by the EDTA titrimetric method using the difference between the calcium content and total hardness (TH). TH measures the sum of the calcium and magnesium. The proce-dures for determining TH and magnesium are presented in this section.

5.7.2 Reagents.

1. Buffer solution. Dissolve 16.9 mg ammonium chloride (NH4Cl, reagent grade) in 143 mL of concentrated ammonium hydroxide (NH4OH); add 1.25 g magnesium salt of EDTA and dilute to 250 mL with distilled water. Keep the solu-tion in a tightly stoppered plastic container.

2. Indicator. Mix together approximately 0.5 g of Eriochrome Black T dye (sodium salt of 1-[1 hydroxy-2-napthylazo]-6-nitro-2-naphthol-4-sulfonic acid) and 100 g reagent-grade NaCl to prepare a dry-powder mixture.

3. Inhibitor. Dissolve 5.0 g Na2S·9H2O (sodium sulfide nonahydrate) or

3.7 g Na2S·5H2O in 100 mL of distilled water. Exclude air with a tightly fitting rubber stopper. This inhibitor deteriorates through air oxidation and should be prepared fresh weekly.

4. Standard EDTA titrant, 0.01M. The same EDTA solution used in the calcium determination may be used (Sec. 5.6.1[Item 3]).

5.7.3 Procedure.

Note: The aliquot of sample taken for the titration should require less than

15 mL of titrant. The duration of titration should not exceed 5 minutes, measured from the time of the buffer addition.

1. Take a 50-mL aliquot or, if necessary, a smaller aliquot, from the diluted filtrate (Sec. 5.6.2[Item 1]) and place it in a tall clear-glass cylinder or casserole.

2. Add 1 to 2 mL of buffer solution (or sufficient buffer to give a pH of 10.0 to 10.1). Add a small amount of powder indicator to produce a moderate color.

Titrate slowly with continuous stirring until the last reddish tinge disappears. The end point should appear as clear blue. Daylight or a daylight fluorescent lamp is highly recommended for observation of the final end point.

Sodium Chloride 11

3. If the reddish tint does not disappear, take another aliquot and add approximately 1 mL of inhibitor to the sample before adding the buffer and indi-cator. This serves as an inhibitor to interfering ions.

5.7.4 Calculation.

M of EDTA × mL EDTA × 105 = mg/L total hardness

(TH) as CaCO3 (Eq 4) mL of aliquot titrated

From Sec. 5.6.3, M of EDTA × (mL EDTA × 4.008) × 104 = mg/L Ca (Eq 5) mL of aliquot titrated

(TH – 2.5 Ca)(2.432)(10–5)(mL aliquot titrated) = percent magnesium (Mg, dry basis) (Eq 6) grams of sample in aliquot

Sec. 5.8 Sulfate

5.8.1 Reagents.

5.8.2 Procedure.

1. To exactly 100 mL of the test solution (Sec. 5.2.6.1 and 5.2.6.2), add 2 mL of 2 percent hydrochloric acid and boil. While the solution is boiling, add a slight excess of barium chloride solution with rapid stirring and set aside at room tempera-ture for approximately 18 hours.

Note: According to recognized authorities, 1-hour digestion of sulfate on a steam bath produces a precipitate of as high a quality as 18 hours standing at room temperature.

2. Filter through a tight quantitative (Whatman No. 42 or equivalent) filter paper and wash precipitate with hot distilled water until a 25-mL portion of the filtrate shows no more than a slight opalescence with silver nitrate.

3. Place the filter paper containing the precipitate in an ignited, cooled, and weighed platinum or dried porcelain crucible and heat slowly over a low flame to char the filter paper without allowing it to catch fire. After complete charring, ignite to constant weight over an ordinary burner with the crucible uncovered, cooling in a desiccator between weighings.

Note: If charring of the paper is too rapid, some of the barium sulfate will be reduced to barium sulfide. If so, moisten the precipitate with concentrated sulfuric acid, carefully heat to expel the acid, and ignite.

12 AWWA B200-17

5.8.3 Calculation.

grams of BaSO4 residue × 41.16 = percent sulfate (SO4, dry basis) (Eq 7) grams of sample in aliquot

Sec. 5.9 Grease, Fat, and Oil

5.9.1 Reagent. N-hexane

5.9.2 Procedure.

1. Weigh approximately 25 to 50 g of the sample, dried to constant weight, and place in a 70-mL Soxhlet tube.

the residue at 110°C to constant weight.

4. Evaporate 100 mL of n-hexane in a tared evaporating dish and subtract the weight of the residue from the weight of the residue obtained in Sec. 5.9.2 (Item 3).

5.9.3 Calculation.

net weight of residue, in grams × 100 = percent grease, fat, and oil (dry basis) (Eq 8) grams of sample

Sec. 5.10 pH Value

5.10.1 Reagent. Freshly boiled and cooled distilled water (avoid reaeration as much as possible).

5.10.2 Procedure.

1. The pH value shall be determined on a 5 percent salt solution at 25°C, prepared by completely dissolving 10 g of salt in approximately 190 mL of distilled water, using gentle stirring.

2. The pH of the solution is determined by using any reliable pH meter equipped with a standard calomel electrode and a glass electrode. The meter and elec-trodes are standardized using pH standard solutions as described in Sec. 4500-H+ of Standard Methods for the Examination of Water and Wastewater. Commercially available buffer tablets, powders, or solutions of tested quality may also be used.

Standardization of the pH meter shall be with buffers in the range of pH 5 to 10, preferably within two pH units of the salt solution being measured.

3. Rinse electrodes with the 5 percent salt solution, discard rinse, then place electrodes into solution. Stir gently for 3 to 4 minutes to allow the electrodes to equilibrate, then read pH value to ±0.1. This equilibration process will occur much more rapidly if the electrodes have been previously stored in a 5 percent salt solu-tion made from reagent-grade sodium chloride.

Sodium Chloride 13

Sec. 5.11 Total Impurities

5.11.1 Water-soluble impurities. The calcium (Ca), magnesium (Mg), and sulfate (SO4) determined by chemical analysis shall be converted to CaSO4, MgSO4, Na2SO4, CaCl2, and MgCl2. Convert sulfate to calcium sulfate (CaSO4) and the unused calcium to calcium chloride (CaCl2). If the sulfate in the sample exceeds the quantity necessary to combine with the calcium, convert the calcium to calcium sulfate (CaSO4) and the unused sulfate first to magnesium sulfate (MgSO4), and the remaining sulfate, if any, to sodium sulfate (Na2SO4). Convert the unused magnesium to magnesium chloride (MgCl2). Each salt impurity shall be reported in percent by weight (dry basis) to the third decimal place.

5.11.2 Conversion factors.

BaSO4 × 0.4115 = SO4

BaSO4 × 0.5832 = CaSO4

BaSO4 × 0.6086 = Na2SO4

Ca × 3967 = CaSO4

Ca × 0.6068 = Mg CaSO4 × 0.2944 = Ca CaSO4 × 0.8153 = CaCl2 CaSO4 × 0.8842 = MgSO4

CaSO4 × 1.0434 = Na2SO4

Mg × 3.9159 = MgCl2 MgCl2 × 1.4296 = CaSO4

MgCl2 × 1.2641 = MgSO4

MgSO4 × 1.1309 = CaSO4

MgSO4 × 0.7911 = MgCl2 MgSO4 × 1.1800 = Na2SO4

SO4 × 1.4173 = CaSO4

5.11.3 Total impurities. The sum of the soluble impurities (either calcium and magnesium sulfate or chloride) plus the insoluble matter (Sec. 5.5) shall con-stitute the total impurities in the salt.

Sec. 5.12 Sodium Chloride Assay

5.12.1 Rock, solar, and compressed solar salt. Report assay by difference to the first decimal place.

5.12.2 Vacuum-granulated and compressed vacuum-granulated salt. Report assay by difference to the second decimal place.

14 AWWA B200-17

5.12.3 Calculation. 100 – percent total impurities = percent NaCl (dry basis).

Sec. 5.13 Notice of Nonconformance

5.13.1 Notice of nonconformance. If the material delivered to the pur-chaser does not meet the chemical, physical, safety, or security requirements of this standard, the purchaser shall provide a notice of nonconformance to the sup-plier within 10 days after receipt of the shipment at the point of destination. If determination of nonconformance of the shipment is based on the chemical and physical characteristics of the material, the results of the purchaser’s tests shall prevail, unless the supplier notifies the purchaser within 5 days of the notice of nonconformance that a retest is desired. On receipt of the request for a retest, the purchaser shall forward to the supplier one of three sealed samples taken in accordance with Sec. 5.2. In the event the results obtained by the supplier do not agree with the results obtained by the purchaser, the other sealed sample shall be forwarded, unopened, for analysis to a referee laboratory agreed on by both parties.

The results of the referee’s analysis shall be accepted as final.

Material not complying with the requirements of this standard and the pur-chaser’s documents may be rejected. Replacement and retesting shall be accom-plished in accordance with the purchaser’s documents.

Because the exact concentration of the active ingredient in specific shipments of some materials can vary within an acceptable range (thereby conforming to the standard), the purchase documents between purchaser and supplier should address treatment of concentration variation.

SECTION 6: DELIVERY

Sec. 6.1 Marking*

6.1.1 Required. Each shipment of material shall be identified as to prod-uct, grade, net weight, name, and address of the manufacturer and the brand name.

Packages or containers shall show a lot number and identification of manufac-turer. All markings on packaged, containerized, or bulk shipments shall conform

* Governmental marking, packaging, and shipping references reflect US requirements. Users of ANSI/AWWA B200 outside the United States should verify applicable local, provincial, and national regulatory requirements. Because of frequent changes in these regulations, all parties should remain informed of possible revisions. Provisions of the purchaser’s document should not preclude compliance with applicable regulations.

Sodium Chloride 15 to applicable laws and regulations, including requirements established by the US Occupational Safety and Health Administration (OSHA).

6.1.2 Optional. Packages may also bear the statement: “Guaranteed by (name of manufacturer) to meet the requirements of ANSI/AWWA B200, Sodium Chloride,” provided that the requirements of this standard are met.

Sec. 6.2 Packaging and Shipping Packaging and shipping of sodium chloride shall conform to current federal, state, and local regulations.

6.2.1 Packaging. Sodium chloride may be shipped in bulk or in 100-lb

(45.4-kg) bags or other commercial packages as specified by the purchaser. Unless otherwise specified, the material shall be packaged in new substantial containers of the type, size, and kind commonly used for the purpose. The containers shall be constructed to ensure acceptance and safe delivery by common or other carriers at the lowest rate to the point of delivery called for in the contract or purchase order.

Packages shall be strong enough to permit coarse crushing of the salt if the material becomes caked during storage.

6.2.2 Bulk container inspection. Bulk or semibulk containers, such as railcars, trailers, and unit hoppers, shall be carefully inspected by the supplier to ensure the absence of contaminating material before loading the sodium chloride.

6.2.3 Net weight. The net weight of packages shall not deviate from the recorded weight by more than ±2.5 percent. If exception is taken to the weight of the material received, the exception shall be based on a certified unit weight of not less than 10 percent of the packages shipped and selected at random from the entire shipment.

6.2.4 Weight certificate. The purchaser may require that bulk shipments be accompanied by certified-weight certificates, or the weights may be checked by the purchaser at the point of delivery.

6.2.5 Security requirements for nonbulk shipments. Packaged product shall be stored, shipped, and delivered in tamper-evident packaging as defined in Section 3, or an alternative method or methods may be agreed on by the manu-facturer and purchaser that provide a reasonable assurance of protection against tampering.

6.2.6 Security requirements for bulk shipments. Bulk quantities of product shall be secured by employing one of the following security measures or a combina-tion of measures:

16 AWWA B200-17

6.2.6.1 Seals. Bulk quantities of product may be sealed with a uniquely numbered tamper-evident seal(s). The seal numbers shall be recorded and disclosed on shipping documents such as the bill of lading. Seals shall be inspected upon receipt of product by the purchaser, and evidence of tampering or removal should be reported to the carrier and supplier.

6.2.6.2 Chain of custody. A continuous chain of custody shall be main-tained between the manufacturer and the purchaser during storage and shipment if so specified by the purchaser.

6.2.6.3 Alternative method. An alternative method or methods may be agreed on by the manufacturer and purchaser that provide reasonable assurance of protection against tampering.

Sec. 6.3 Affidavit of Compliance The purchaser may require either (1) an affidavit from the manufacturer that the sodium chloride complies with applicable requirements of this standard or (2) a certified analysis of the material at the time of delivery detailing the desired item.

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